CN102127741A - Method for preparing high-purity molybdenum target for thin film solar cell - Google Patents
Method for preparing high-purity molybdenum target for thin film solar cell Download PDFInfo
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- CN102127741A CN102127741A CN2011100360018A CN201110036001A CN102127741A CN 102127741 A CN102127741 A CN 102127741A CN 2011100360018 A CN2011100360018 A CN 2011100360018A CN 201110036001 A CN201110036001 A CN 201110036001A CN 102127741 A CN102127741 A CN 102127741A
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Abstract
The invention aims to provide a method for preparing a high-purity molybdenum target for a thin film solar cell, which aims to improve the quality of the solar cell. The process flow comprises the following steps of: baking ammonium molybdate serving as a raw material to prepare Mo3; introducing high-purity hydrogen to primarily reduce the Mo3 into Mo2 at the temperature of between 450 and 600 DEG C; introducing the high-purity hydrogen to secondarily reduce the Mo2 into Mo at the temperature of between 950 and 1,050 DEG C; mixing materials; sieving; performing isostatic pressing; charging and discharging the high-purity hydrogen for multiple times and then sintering in a medium frequency induction furnace at the temperature of between 1,950 and 2,000 DEG C; performing high-power electron beam smelting and purification; forging at the temperature of between 1,400 and 1,450 DEG C; performing hot rolling at the temperature of between 1,350 and 1,450 DEG C; performing thermal annealing at the temperature of between 900 and 1,000 DEG C; machining; performing ultrasonic cleaning; braze-welding a target holder; and testing and examining performance. The method has the advantages that: the high-purity molybdenum target for the thin film solar cell has the characteristics of high purity, high density and high uniformity, the utilization rate of a sputtering target is greatly improved, and the method has extremely high value when applied to a solar cell industry.
Description
Technical field
The invention belongs to energy utilization technology field, particularly technical field of solar cell manufacturing.
Background technology
Thin-film solar cells is the multi-layer film structure assembly, such as, CIGS (copper-indium-galliun-selenium) thin-film solar cells mainly is made up of substrate (normally glass), dorsum electrode layer (normally Mo), absorption layer (p-CIGS), buffer layer (normally n-CdS), transparency conducting layer (normally ZnO or Al doping ZnO bilayer structure), upper electrode layer (being generally Ni/Al) and antireflection layer (normally MgF2).Here, dorsum electrode layer is one deck molybdenum film (0.5-1.5 μ m is thick) as thin as a wafer, and it is to adopt the technology of sputtered film to be splashed in the substrate by molybdenum target to form.
Physical vapor deposition (PVD) is a technical matters the most key in the coating technique, and PVD is one of most important starting material in the membrane prepare course of processing with the splash-proofing sputtering metal target.The quality quality of splash-proofing sputtering metal target plays an important role to the capability and performance of film.At present, thin-film solar cells is mainly overseas enterprise with the molybdenum target material and monopolizes, though China is the starting material big producing country of molybdenum target material, owing to reasons such as technology, does not manufacture the target of high quality, high stable performance always.The present main dependence on import of the employed target of China's high-end product.The technology of the high-end molybdenum target material of world production and market are a few countries monopolizations such as Germany, Japan, the U.S..
Generally, the purity of molybdenum target, density and homogeneity of structure are directly connected to the quality and the thickness evenness of plated film, and then have influence on electrode performance the sputter important influence.Simultaneously because dorsum electrode layer is one deck molybdenum film as thin as a wafer, even trickle inclusion all may impact the quality of film in the film, nonmetallic impurity thing especially.These strict demands to coating quality are reflected on the sputtering target, just require the weave construction of sputtering target material and chemical purity should meet corresponding technology.
How to suppress that the generation of particulate is an important factor of guaranteeing coating quality in the sputter procedure.In the process of sputter coating, so-called particulate is meant large-sized target particle or the particulate that produces when sputtering target is subjected to high-energy ion bombardment, or the particulate that the film material is subjected to secondary electron to bombard out to form after the film forming.The generation of these particulates for film forming quality very big influence is arranged, especially require very harsh microelectronic industry for membrane quality.The one of the main reasons of these particulates generations is because the compact structure of sputtering target material is not enough, and the gas that exists in target internal void during sputter release is suddenly caused.The most normal sputtering target made from powder technology (as hot compacting, sintering, pyrolytic coating moulding etc.) that occurs in of the phenomenon of this particulate that splashes.Therefore, how improving the sputtering target density also is one of important technology problem.
In the planar magnetic control sputtering process, because crossed electric and magnetic field is to the interactively of plasma sputter, sputtering target will produce inhomogeneous erosion (Erosion) phenomenon in sputter procedure, thereby the utilization ratio that causes sputtering target material is general usually low, and the utilization ratio of rectangle sputtering target (weight percent) is at 25%-40%.Need more frequent replacing target in the production.Therefore the utilization ratio that how to improve sputtering target material is subjected to greatly paying close attention to.
Summary of the invention
The object of the invention provides a kind of preparation method of high-purity molybdenum target for thin-film solar cell, to improve the quality of solar cell.
Thin-film solar cells high purity molybdenum target preparation method is characterized in that according to following flow implementation:
Raw material ammonium molybdate → roasting prepares Mo
3→ feed high-purity hydrogen once to be reduced into Mo at temperature 450-600 ℃
2→ to feed high-purity hydrogen once more be that 950-1050 ℃ of secondary reduction becomes Mo → batch mixing → screening → isostatic pressing → through medium-frequency induction furnace sintering after repeatedly charging and discharging high-purity hydrogen, purification → 1400-1450 ℃ forging → 1350-1450 ℃ hot rolling → 900-1000 ℃ of heat-treatment of annealing → mechanical workout → ultrasonic cleaning → soldering target holder → performance test and check of sintering temperature 1950-2000 ℃ → great-power electronic bundle melting in temperature.
Advantage of the present invention is the characteristics that high-purity molybdenum target for thin-film solar cell has high purity, high-density and good homogeneous, has greatly improved the utilization ratio of sputtering target material, is applied to the solar cell industry and has very high value.
Innovative point of the present invention comprises: the one, and repeatedly purification techniques innovation of high-purity hydrogen adopts high-purity hydrogen reduction-oxidation molybdenum to improve product purity.When the Medium frequency induction sintering, adopt in specific temperature and to fill hydrogen three times, the method that vacuumizes for three times improve molybdenum base purity, thereby the project product of making reaches design requirements.The 2nd, the application innovation of electron beam melting purification techniques is applied to the electron beam cold hearth melting technology in the processing of molybdenum target material, and smelting temperature can reach more than 3000 ℃, and vacuum tightness reaches 10 in the stove
-5Pa, carbon oxygen fully reacts under the vacuum that is highly advantageous to, and can obtain good deoxidation effect.In fusion process, other impurity except that molybdenum can both be overflowed with the metal vapors form, can obtain the high purity Mo through twice melting usually.The 3rd, the innovation of aximal deformation value rolling technique, adopting power is 2000 tons of milling trains of 1250KW, when rolling, draught per pass is greater than 30%-50% (generally below 20%), the aximal deformation value hot rolling guarantees that its weave construction and product performance are good, and grain-size is below 50 microns.
Embodiment
Thin-film solar cells high purity molybdenum target preparation method, implement according to following steps: raw material ammonium molybdate → roasting prepares Mo
3→ feed high-purity hydrogen once to be reduced into Mo at temperature 450-600 ℃
2→ to feed high-purity hydrogen once more be that 950-1050 ℃ of secondary reduction becomes Mo → batch mixing → screening → isostatic pressing → through medium-frequency induction furnace sintering after repeatedly charging and discharging high-purity hydrogen, purification → 1400-1450 ℃ forging → 1350-1450 ℃ hot rolling → 900-1000 ℃ of heat-treatment of annealing → mechanical workout → ultrasonic cleaning → soldering target holder → performance test and check of sintering temperature 1950-2000 ℃ → great-power electronic bundle melting in temperature.Roasting prepares Mo
3Shi Wendu is controlled at 500-600 ℃, simultaneously material by the stoving oven flow according to being no more than 100 kilograms/1 hour throughput.Power was not less than 1200KW when the melting of great-power electronic bundle was purified.Smelting temperature is not less than 3000 ℃, vacuum tightness 10 in the stove
-5More than the Pa.During the Medium frequency induction sintering, adopt and fill hydrogen at least three times, the method that vacuumizes for three times improves molybdenum base purity.Adopting power during hot rolling is the above milling train that is not less than 2000 tons of pressure of 1250KW, and when rolling, draught per pass is greater than the aximal deformation value hot rolling of 30%-50%.
The present invention has made improvement to existing target aspect following:
1, purity: well-known, the electroconductibility of metal and the purity of material have substantial connection, the foreign matter content of reduction metal molybdenum, and the content of oxygen especially can improve the heat conduction and the conductivity of molybdenum back electrode.It is O≤0.004% that molybdenum target of the present invention has the oxygen level standard, Mo 〉=99.97% (metal content), and also other impurity is according to following table control (attached common molybdenum plate data simultaneously)
2, density: because molybdenum target adopts the powder metallurgy manufacturing, if inappropriate technology can reduce the density of molybdenum target, serious words can also can cause target tissue looseness, influence the target quality.The described molybdenum target of this patent improves target density by the gross distortion working modulus and eliminates tissue looseness's defective of sintered products.Density can reach 10.2g/cm
3.
3, homogeneity of structure: molybdenum target of the present invention has uniform heat-treated sturcture, is beneficial to obtain the equally distributed plated film of thickness.
Simultaneously, the present invention also uses equipment new innovation.
Molybdenum divides reduction to carry out in four pipe electric reduction furnaces, adopts the hydrogen (containing moisture below 0.5g/m3) through thorough drying, and reduction temperature rises to 920 ℃ of discharge ends for about 500 ℃ along the boiler tube length direction from feed end.The factor that influences the molybdenum powder quality mainly contains raw materials quality, dress boat situation, reduction temperature, hydrogen flowing quantity and humidity, material at residing time in furnace.The purity of raw material molybdenum dioxide has determined the purity of product molybdenum powder.Charge amount, bed of material thickness, material tightness in the reduction boat all can have influence on the infiltration of hydrogen, the eliminating of reduction aqueous vapor, thereby also can have influence on the quality of product molybdenum powder.Reduction temperature is low, and reduction reaction is incomplete, and speed of response is slow, gained molybdenum powder oxygen level height, fine size; The reduction temperature height then in contrast.Hydrogen humidity is big, and the molybdenum powder oxygen level increases, coarse size; Hydrogen flowing quantity is big, and reduction reaction speeds up, and the molybdenum powder oxygen level descends, but material that is pulled away and calorific loss increase.Material is long at residing time in furnace, and product molybdenum powder oxygen level descends and the granularity chap.In reduction process, manage to avoid the quality of bringing and prevent molybdenum powder oxidation when cooling also can raising product molybdenum powder into of other impurity.The molybdenum powder of reduction output will in time sieve and close to be criticized.
The vacuum induction sintering oven is to fill after vacuumizing under the hydrogen shield state; utilize the principle of Frequency Induction Heating; make the tungsten crucible that is in the coil produce high temperature; be transmitted on the workpiece by thermal radiation; vacuum outgas is meant the process that removes gaseous impurities in the metal under vacuum condition; be actually and reduce the solubleness of gaseous impurities in metal; therefore improve the vacuum tightness of system; just be equivalent to reduce the dividing potential drop of gas; also can reduce the solubleness of gas in metal, and the portion gas impurity that surpasses solubleness can be overflowed from metal just and be removed.It is many more with the number of times that vacuumizes to fill hydrogen, and refining effect is good more.
Electron beam melting furnace is the specific equipment of high temperature refractory melting and purification of metals.Under high vacuum condition, negative electrode is launched electronics owing to the effect of high-voltage electric field is heated, and electronics compiles bunchy, and electron beam is under the effect of acceleration voltage, with high speed anode motion, after passing anode, under the effect of focusing coil and deflector coil, bombard exactly on the end ingot and material in the crystallizer, end ingot is melted forms the molten bath, material also constantly is melted and drops onto in the molten bath, thereby realizes fusion process, electron beam melting principle that Here it is.
Electron beam melting is to carry out under high vacuum state, temperature of superheat height during melting, and it is long to keep the liquid time, makes the concise purification effect of metal obtain fully effectively carrying out, and the material production degassing, deoxidation, metallic impurity volatilization, does not melt impurity come-up etc.Under draw in the ingot casting process, molten impurity come-up is enriched in head of ingot top, refractory metal is enriched in outside surface, removes the ingot casting top and peel exterior skin off to obtain high-purity cast metals.
Claims (6)
1. thin-film solar cells is characterized in that according to following flow implementation with high purity molybdenum target preparation method:
Raw material ammonium molybdate → roasting prepares Mo
3→ feed high-purity hydrogen once to be reduced into Mo at temperature 450-600 ℃
2→ to feed high-purity hydrogen once more be that 950-1050 ℃ of secondary reduction becomes Mo → batch mixing → screening → isostatic pressing → through medium-frequency induction furnace sintering after repeatedly charging and discharging high-purity hydrogen, purification → 1400-1450 ℃ forging → 1350-1450 ℃ hot rolling → 900-1000 ℃ of heat-treatment of annealing → mechanical workout → ultrasonic cleaning → soldering target holder → performance test and check of sintering temperature 1950-2000 ℃ → great-power electronic bundle melting in temperature.
2. thin-film solar cells according to claim 1 is characterized in that with high purity molybdenum target preparation method roasting prepares Mo
3Shi Wendu is controlled at 500-600 ℃, simultaneously material by the stoving oven flow according to being no more than 100 kilograms/1 hour throughput.
3. thin-film solar cells according to claim 1 high purity molybdenum target preparation method, power is not less than 1200KW when it is characterized in that great-power electronic bundle melting purification.
4. thin-film solar cells according to claim 1, adopts and fills hydrogen at least three times when it is characterized in that the Medium frequency induction sintering with high purity molybdenum target preparation method, the method that vacuumizes for three times, raising molybdenum base purity
5. according to claim 1 or 3 described thin-film solar cells high purity molybdenum target preparation method, smelting temperature is not less than 3000 ℃ when it is characterized in that great-power electronic bundle melting purification, vacuum tightness 10 in the stove
-5More than the Pa.
6. thin-film solar cells according to claim 1 high purity molybdenum target preparation method, adopting power when it is characterized in that hot rolling is the above milling train that is not less than 2000 tons of pressure of 1250KW, and when rolling, draught per pass is greater than the aximal deformation value hot rolling of 30%-50%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102259182A (en) * | 2011-07-22 | 2011-11-30 | 中国科学院金属研究所 | Method for preparing high-performance molybdenum cake material by using smelting method |
| CN102628107A (en) * | 2012-04-18 | 2012-08-08 | 吉安市荣泰电讯科技有限公司 | Method for secondarily purifying copper through vacuum induction electron beam melting |
| CN102983219A (en) * | 2012-12-03 | 2013-03-20 | 深圳先进技术研究院 | Preparation method of thin-film solar cell component |
| CN103114213A (en) * | 2012-11-08 | 2013-05-22 | 宝鸡市博信金属材料有限公司 | Method for preparing high-purity molybdenum for sapphire growth furnace |
| CN103132033A (en) * | 2013-03-26 | 2013-06-05 | 金堆城钼业股份有限公司 | Method for preparing molybdenum target |
| CN103658653A (en) * | 2012-09-24 | 2014-03-26 | 上海六晶金属科技有限公司 | One-time sintering method of pure molybdenum metal sheet green pressing |
| CN103805952A (en) * | 2013-12-12 | 2014-05-21 | 株洲硬质合金集团有限公司 | Large-sized high purity tungsten target and production method thereof |
| CN104520466A (en) * | 2012-05-09 | 2015-04-15 | H·C·施塔克公司 | Multi-block sputtering target with interface portions and associated methods and articles |
| CN111971804A (en) * | 2018-02-15 | 2020-11-20 | 伊利诺斯工具制品有限公司 | Method and apparatus for providing closed loop control in a solar cell production system |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102259182A (en) * | 2011-07-22 | 2011-11-30 | 中国科学院金属研究所 | Method for preparing high-performance molybdenum cake material by using smelting method |
| CN102628107A (en) * | 2012-04-18 | 2012-08-08 | 吉安市荣泰电讯科技有限公司 | Method for secondarily purifying copper through vacuum induction electron beam melting |
| CN104520466A (en) * | 2012-05-09 | 2015-04-15 | H·C·施塔克公司 | Multi-block sputtering target with interface portions and associated methods and articles |
| CN104520466B (en) * | 2012-05-09 | 2017-06-27 | H·C·施塔克公司 | Polylith sputtering target and correlation technique and article with interface portion |
| CN103658653A (en) * | 2012-09-24 | 2014-03-26 | 上海六晶金属科技有限公司 | One-time sintering method of pure molybdenum metal sheet green pressing |
| CN103114213A (en) * | 2012-11-08 | 2013-05-22 | 宝鸡市博信金属材料有限公司 | Method for preparing high-purity molybdenum for sapphire growth furnace |
| CN102983219A (en) * | 2012-12-03 | 2013-03-20 | 深圳先进技术研究院 | Preparation method of thin-film solar cell component |
| CN102983219B (en) * | 2012-12-03 | 2015-04-15 | 深圳先进技术研究院 | Preparation method of thin-film solar cell component |
| CN103132033A (en) * | 2013-03-26 | 2013-06-05 | 金堆城钼业股份有限公司 | Method for preparing molybdenum target |
| CN103132033B (en) * | 2013-03-26 | 2016-03-16 | 金堆城钼业股份有限公司 | A kind of method preparing molybdenum target |
| CN103805952A (en) * | 2013-12-12 | 2014-05-21 | 株洲硬质合金集团有限公司 | Large-sized high purity tungsten target and production method thereof |
| CN111971804A (en) * | 2018-02-15 | 2020-11-20 | 伊利诺斯工具制品有限公司 | Method and apparatus for providing closed loop control in a solar cell production system |
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Application publication date: 20110720 |